CN106008618A - Preparation method of salidroside - Google Patents
Preparation method of salidroside Download PDFInfo
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- CN106008618A CN106008618A CN201610462599.XA CN201610462599A CN106008618A CN 106008618 A CN106008618 A CN 106008618A CN 201610462599 A CN201610462599 A CN 201610462599A CN 106008618 A CN106008618 A CN 106008618A
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- rhodioside
- radix rhodiolae
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H15/00—Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
- C07H15/18—Acyclic radicals, substituted by carbocyclic rings
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
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Abstract
The invention belongs to the technical field of drug extraction and particularly relates to a preparation method of salidroside. The method comprises steps as follows: 1) rhodiola is taken, crushed and treated under high pressure, and pasty slurry is obtained; 2) ultrasonic wave extraction and ultrafiltration are performed, and filtrate is collected for standby use; 3) the filtrate is compressed, an ethanol solution is added for precipitation, and precipitates are obtained through centrifugation; 4) washing is performed twice, vacuum drying is performed, and salidroside is obtained. According to the method, the oxidation resistance and the anti-aging efficacy of salidroside can be effectively improved.
Description
Technical field
The invention belongs to extract drugs technical field, particularly to the preparation method of a kind of rhodioside.
Background technology
Radix Rhodiolae (Rhodiola) is Crassulaceae rhodiola perennial herb or semishrub plant, is precious
One of dilute medicinal plants, is described as " plateau Radix Ginseng ".This platymiscium the most about 90 kinds in the whole world,
China is distributed kind more than 70, main product in North China, northeast, southwest, the area such as northwest and Central China.Its chemistry
Composition mainly has flavonoid, butyl alcohol, Radix Rhodiolae (Salidroside), sitosterol, organic acid, volatilization
Oil, polysaccharide, fat, protein etc..Wherein, rhodioside and tyrosol thereof are that Radix Rhodiolae is main
Active ingredient, is also to evaluate Radix Rhodiolae and the most important index of extract thereof.Modern pharmacology research card
Real, Radix Rhodiolae extract have defying age, antitumor, antiviral, antibacterial, anti-hypoxia, resisting fatigue,
Radioprotective, antioxidation, analgesia, to various active such as nervus centralis and hormonal system two-ways regulations,
And there is the least side effect.
Study a kind of method improving rhodioside non-oxidizability and senile-resistant efficacy, be going out of the present invention
Send out point.
Summary of the invention
The technical problem to be solved is to provide the preparation method of a kind of rhodioside, the method
Rhodioside non-oxidizability and senile-resistant efficacy can be effectively improved.
For achieving the above object, technical scheme to be solved by this invention is:
The present invention provides the preparation method of a kind of rhodioside, comprises the following steps:
1) taking Radix Rhodiolae to pulverize, put in pressure pan, the methanol adding Radix Rhodiolae weight 8～13 times is molten
Liquid, is forced into 26～30MPa and carries out HIGH PRESSURE TREATMENT 3～7min, release, obtain paste serous material；
2) add Radix Rhodiolae weight 4～the methanol solution of 8 times to paste serous material, frequency be 80～
Ultrasonic extraction 15～25min under 160kHz, ultrafiltration, collect filtrate standby；
3) filtrate is compressed to the 1/4～1/2 of original filtrate volume, adds ethanol solution precipitation, from
Gains in depth of comprehension precipitate；
4) carry out the anhydrous ethyl acetate of precipitation Radix Rhodiolae proper mass 5～9 times washing for the first time, then
Carry out second time with the absolute methanol of Radix Rhodiolae proper mass 3～6 times to wash, vacuum drying, obtain red scape
It glycosides.
Preferably, step 1 of the present invention) and step 2) the volumetric concentration of methanol solution be 60～
75%.
Preferably, step 2 of the present invention) ultrafiltration time aperture be 10～15nm film.
Preferably, step 3 of the present invention) the volumetric concentration of ethanol solution be 80～90%.
Preferably, step 3 of the present invention) under 3000～4000r/min rotating speeds, it is centrifuged 5～8min.
Radix Rhodiolae of the present invention is dry root and the rhizome of Crassulaceae Radix Rhodiolae.
Compared to existing technology, the beneficial effects of the present invention is:
1, the present invention is before ultrasonic extraction, and advanced horizontal high voltage processes, and is conducive to improving ultrasonic extraction
Efficiency, additionally it is possible to improve the extraction ratio of rhodioside and purity, improve the anti-of rhodioside for the later stage
Oxidation and activity of fighting against senium do basis.
2, the present invention uses ultrasonic extraction, while the active substance of protection rhodioside, moreover it is possible to
Enough interrupt the main chain of rhodioside, reduce relative molecular mass, expose more antioxidation and defying age
Group, thus reach to improve antioxidation and the effect of activity of fighting against senium of rhodioside.
3, the rhodioside purity that the inventive method prepares is high, reaches 99.2%, and extraction ratio is the most existing
Technology is had to improve 6.3～9.6%.
4, through test, the rhodioside that hinge structure prepares, the inventive method prepares
Rhodioside to DPPH suppression ratio improve 29.3～36.2%, ABTS+Suppression ratio improve 33.6～
37.2%, reducing power improves 26.9～31.8%, and total economic value significantly improves.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described, but the invention is not limited in that these are real
Execute example.
Embodiment 1
1) taking Radix Rhodiolae to pulverize, put in pressure pan, adding 13 times of volumetric concentrations of Radix Rhodiolae weight is
The methanol solution of 75%, is forced into 26MPa and carries out HIGH PRESSURE TREATMENT 7min, release, obtain paste serous material；
2) adding 4 times of volumetric concentrations of Radix Rhodiolae weight to paste serous material is the methanol solution of 75%,
Frequency is ultrasonic extraction 15min under 160kHz, is the membrane ultrafiltration of 15nm with aperture, collects filtrate standby
With；
3) filtrate being compressed to the 1/4 of original filtrate volume, adding volumetric concentration is that 90% ethanol is molten
Liquid precipitate, under 3000r/min rotating speed, centrifugal 8min must precipitate；
4) carry out the anhydrous ethyl acetate of precipitation Radix Rhodiolae proper mass 5 times washing, then use for the first time
The absolute methanol that Radix Rhodiolae proper mass is 6 times carries out second time and washs, and vacuum drying obtains rhodioside.
Embodiment 2
1) taking Radix Rhodiolae to pulverize, put in pressure pan, adding 12 times of volumetric concentrations of Radix Rhodiolae weight is
The methanol solution of 71%, is forced into 27MPa and carries out HIGH PRESSURE TREATMENT 6min, release, obtain paste serous material；
2) adding 5 times of volumetric concentrations of Radix Rhodiolae weight to paste serous material is the methanol solution of 71%,
Frequency is ultrasonic extraction 18min under 140kHz, is the membrane ultrafiltration of 14nm with aperture, collects filtrate standby
With；
3) filtrate being compressed to the 1/3 of original filtrate volume, adding volumetric concentration is that 88% ethanol is molten
Liquid precipitate, under 3200r/min rotating speed, centrifugal 6min must precipitate；
4) carry out the anhydrous ethyl acetate of precipitation Radix Rhodiolae proper mass 6 times washing, then use for the first time
The absolute methanol that Radix Rhodiolae proper mass is 4 times carries out second time and washs, and vacuum drying obtains rhodioside.
Embodiment 3
1) taking Radix Rhodiolae to pulverize, put in pressure pan, adding 11 times of volumetric concentrations of Radix Rhodiolae weight is
The methanol solution of 68%, is forced into 28MPa and carries out HIGH PRESSURE TREATMENT 5min, release, obtain paste serous material；
2) adding 6 times of volumetric concentrations of Radix Rhodiolae weight to paste serous material is the methanol solution of 68%,
Frequency is ultrasonic extraction 20min under 120kHz, is the membrane ultrafiltration of 13nm with aperture, collects filtrate standby
With；
3) filtrate being compressed to the 1/3 of original filtrate volume, adding volumetric concentration is that 85% ethanol is molten
Liquid precipitate, under 3500r/min rotating speed, centrifugal 7min must precipitate；
4) carry out the anhydrous ethyl acetate of precipitation Radix Rhodiolae proper mass 7 times washing, then use for the first time
The absolute methanol that Radix Rhodiolae proper mass is 5 times carries out second time and washs, and vacuum drying obtains rhodioside.
Embodiment 4
1) taking Radix Rhodiolae to pulverize, put in pressure pan, adding 9 times of volumetric concentrations of Radix Rhodiolae weight is 64%
Methanol solution, be forced into 29MPa and carry out HIGH PRESSURE TREATMENT 4min, release, obtain paste serous material；
2) adding 7 times of volumetric concentrations of Radix Rhodiolae weight to paste serous material is the methanol solution of 64%,
Frequency is ultrasonic extraction 23min under 100kHz, is the membrane ultrafiltration of 11nm with aperture, collects filtrate standby
With；
3) filtrate being compressed to the 1/2 of original filtrate volume, adding volumetric concentration is that 82% ethanol is molten
Liquid precipitate, under 3800r/min rotating speed, centrifugal 6min must precipitate；
4) carry out the anhydrous ethyl acetate of precipitation Radix Rhodiolae proper mass 8 times washing, then use for the first time
The absolute methanol that Radix Rhodiolae proper mass is 4 times carries out second time and washs, and vacuum drying obtains rhodioside.
Embodiment 5
1) taking Radix Rhodiolae to pulverize, put in pressure pan, adding 8 times of volumetric concentrations of Radix Rhodiolae weight is 60%
Methanol solution, be forced into 30MPa and carry out HIGH PRESSURE TREATMENT 3min, release, obtain paste serous material；
2) adding 8 times of volumetric concentrations of Radix Rhodiolae weight to paste serous material is the methanol solution of 60%,
Frequency is ultrasonic extraction 25min under 80kHz, is the membrane ultrafiltration of 10nm with aperture, collects filtrate standby
With；
3) filtrate being compressed to the 1/4 of original filtrate volume, adding volumetric concentration is that 80% ethanol is molten
Liquid precipitate, under 4000r/min rotating speed, centrifugal 5min must precipitate；
4) carry out the anhydrous ethyl acetate of precipitation Radix Rhodiolae proper mass 9 times washing, then use for the first time
The absolute methanol that Radix Rhodiolae proper mass is 3 times carries out second time and washs, and vacuum drying obtains rhodioside.
Test example: the senile-resistant efficacy of the rhodioside that the inventive method prepares
1, model and be administered
Take Wistar rat 50, be randomly divided into 4 groups (normal group, subacute aging animal groups, red
Herba hylotelephii erythrosticti glycosides A group and rhodioside B group), often group 10.Except normal group Wistar rat nape portion skin
Outside hemostasis normal saline, remaining respectively organizes Wistar rat neck dorsal sc injection D-galactose
100mg/kg, l time/d, injects 42d continuously, to build Wistar rat aging model.Meanwhile, A
Group (commercially available rhodioside) and B group (rhodioside that embodiment 3 prepares) are by 30mL/kg every day
Dosage to Wistar rat oral gavage rhodioside juice, normal group and model group gavage normal saline.
2, SOD in serum, MDA and GSH-Px survey
After 42d last is administered 2h, take blood, blood in Wistar rat eye rear vein beard capillary tube
After sample stands, 3500r/min is centrifuged 10min, takes serum and strictly illustrates to be measured by test kit.
1, cerebral tissue LPF measures
After Wistar rat extracting blood, rapid cervical dislocation is put to death, and cuts cerebral tissue, with 4 DEG C of normal saline
Blot with filter paper after flushing ,-20 DEG C of freezen protective.During mensuration, brain tissue homogenate, 3000r/min at 4 DEG C
Centrifugal 10min, takes supernatant and strictly illustrates to be measured by test kit.
2, result of the test
Each group rat blood serum SOD, MDA, GSH-Px and cerebral tissue LPF changes of contents
Above-mentioned test understands, and rhodioside prepared by the inventive method can effectively suppress serum MDA and brain
SOD and GSH-Px vigor in tissue LPF generation, reinforcement, has good senile-resistant efficacy, phase
The rhodioside preparing prior art, senile-resistant efficacy significantly improves.
Claims (5)
1. the preparation method of a rhodioside, it is characterised in that comprise the following steps:
1) taking Radix Rhodiolae to pulverize, put in pressure pan, the methanol adding Radix Rhodiolae weight 8～13 times is molten
Liquid, is forced into 26～30MPa and carries out HIGH PRESSURE TREATMENT 3～7min, release, obtain paste serous material；
2) add Radix Rhodiolae weight 4～the methanol solution of 8 times to paste serous material, frequency be 80～
Ultrasonic extraction 15～25min under 160kHz, ultrafiltration, collect filtrate standby；
3) filtrate is compressed to the 1/4～1/2 of original filtrate volume, adds ethanol solution precipitation, from
Gains in depth of comprehension precipitate；
4) carry out the anhydrous ethyl acetate of precipitation Radix Rhodiolae proper mass 5～9 times washing for the first time,
Carry out second time with the absolute methanol of Radix Rhodiolae proper mass 3～6 times again to wash, vacuum drying, obtain red
Herba hylotelephii erythrosticti glycosides.
The preparation method of rhodioside the most according to claim 1, it is characterised in that: described step
Rapid 1) and step 2) the volumetric concentration of methanol solution be 60～75%.
The preparation method of rhodioside the most according to claim 1, it is characterised in that: described step
Rapid 2) during ultrafiltration, aperture is the film of 10～15nm.
The preparation method of rhodioside the most according to claim 1, it is characterised in that: described step
Rapid 3) volumetric concentration of ethanol solution is 80～90%.
The preparation method of rhodioside the most according to claim 1, it is characterised in that: described step
Rapid 3) under 3000～4000r/min rotating speeds, it is centrifuged 5～8min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610462599.XA CN106008618B (en) | 2016-06-22 | 2016-06-22 | A kind of preparation method of rhodioside |
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| CN201610462599.XA CN106008618B (en) | 2016-06-22 | 2016-06-22 | A kind of preparation method of rhodioside |
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| CN106008618A true CN106008618A (en) | 2016-10-12 |
| CN106008618B CN106008618B (en) | 2019-01-04 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107602635A (en) * | 2017-10-19 | 2018-01-19 | 阜康市天鼎生物科技有限公司 | The high efficiency extraction separating technology of rhodioside in a kind of rhodiola root |
| CN107857784A (en) * | 2017-12-18 | 2018-03-30 | 四川合盛生物科技有限公司 | A kind of method that rhodioside is extracted from rhodiola root |
| CN108271984A (en) * | 2018-01-02 | 2018-07-13 | 中国农业科学院农产品加工研究所 | Rhodiola root solid beverage and preparation method thereof |
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| CN103923132A (en) * | 2014-04-16 | 2014-07-16 | 安徽博格生物科技有限公司 | Ultrasonic extraction technology for salidroside in natural Rhodiola rosea |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103923132A (en) * | 2014-04-16 | 2014-07-16 | 安徽博格生物科技有限公司 | Ultrasonic extraction technology for salidroside in natural Rhodiola rosea |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107602635A (en) * | 2017-10-19 | 2018-01-19 | 阜康市天鼎生物科技有限公司 | The high efficiency extraction separating technology of rhodioside in a kind of rhodiola root |
| CN107857784A (en) * | 2017-12-18 | 2018-03-30 | 四川合盛生物科技有限公司 | A kind of method that rhodioside is extracted from rhodiola root |
| CN108271984A (en) * | 2018-01-02 | 2018-07-13 | 中国农业科学院农产品加工研究所 | Rhodiola root solid beverage and preparation method thereof |
| CN108271984B (en) * | 2018-01-02 | 2021-05-11 | 中国农业科学院农产品加工研究所 | Rhodiola root solid beverage and preparation method thereof |
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| CN106008618B (en) | 2019-01-04 |
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Effective date of registration: 20181115 Address after: 541004 pavement 1-4 and 2-4, 1 Tung ring new village, Putuo Road, East Ring Road, Qixing District, Guilin, the Guangxi Zhuang Autonomous Region Applicant after: GUILIN RONGTONG TECHNOLOGY CO., LTD. Address before: 541002 No. 1 Jing Ping Road, Xiangshan District, Guilin, the Guangxi Zhuang Autonomous Region. Applicant before: Gao Feng |
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Effective date of registration: 20211213 Address after: 264205 No. 68, Qilu Avenue, economic and Technological Development Zone, Weihai City, Shandong Province Patentee after: WEIHAI ZIGUANG BIOLOGICAL TECHNOLOGY DEVELOPMENT CO.,LTD. Address before: 541004 pavement 1-4 and 2-4, 1 Tung ring new village, Putuo Road, East Ring Road, Qixing District, Guilin, the Guangxi Zhuang Autonomous Region Patentee before: GUILIN RONGTONG TECHNOLOGY Co.,Ltd. |
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